Process of distillation of crude oils from pine-wood.



No. 766,717. PATENTED AUG. 2, 1904. J. G. MALLONEE.

PROCESS OF DISTILLATION 0F CRUDE OILS PROM .PINE WOOD.

APPLICATION FILED JULY 1a. 1903.

NO MODEL. 2 SHEETS-SHEET 1.

Wits twee J PATENTBD AUG. 2, 1904.

J. O. MALLONEE. PROCESS OF DISTILLATION OP ORUDE OILS FROM PINE WOOD.

APPLIOATION FILED JULY 18, 1903.

2 SHEETS-SHEET 2.

NO MODEL.

woewto'c UNITED STATES Patented August 2, 1904.

PATENT OEEIcE.

JOHN OAPLES MALLONEE, OF CHARLOTTE, NORTH CAROLINA, ASSIGNOR OF ONE-HALF TO JOHN JEFFERSON MALLONEE, OF ORIOHTON, ALA- BAM A.

PROCESS OF DISTILLATION OF CRUDE OILS FROM PINE-WOOD.

SPECIFICATION forming" part of Letters Patent No. 766,717, dated August 2, 1904.

Application filed July 18,1903. Serial No. 166,137. (No specimens.)

To all whmn it 71mg concern.-

Re it known that I, J on): GAPLES lMALLONEE, a citizen of the United States, residing at Charlotte, in the county of Mecklenburg and State of North Carolina, have invented new and useful Improvementsin Processes of Distillation of Crude Oils from Pine-\Vood, of which the following is a specification.

My invention relates to improvements in IO the art of distillation of crude oils from pinewood; and the object of the same is to provide an improved method of heating the wood to obtain the crude oil and afterward fractionally distilling the said oil to obtain turpentine 5 and oil of maximum purity with minimum labor and waste.

The method heretofore commonly used consisted in reducing the wood by means of lire acting on the closed retort containing the wood and then catching and condensing all the distillate in one bulk and running it into one receptacle. The contents of the receptacle were then refined by the use of an ordinary still. This mode of procedure is obviously 5 very expensive and wasteful, as it necessitates the handling of oils of all gravities as one product.

By my method the distillate is divided into three fractions of graduated specific gravities,

3 and these fractions are each treated separately to obtain the turpentine, oils, tar, &c.

The apparatus used in carrying out my process is fully described in this specification, but not claimed, as it forms the subject-matter of a separate application for a patent filed of even date herewith and serially numbered 166,139.

In the drawings which accompany this specification and form a part thereof, Figure 1 is a 4 side elevation of the retort and condenser with the parts broken away. Fig. 2 is a side elevation of my distilling apparatus with parts broken away. Fig. 3 is a detail showing means for applying a spray to the column 13. v

In the said accompanying drawings, the

numeral 1 designates a retort heated by a furnace 2. A pipe 3, connected to a source of steam under pressure, extends into the retort 1 and is provided with a spray 3. An outletpipe 1 is connected to the top of the retort 1 5 and to a condenser 5,which is in turn connected to a receptacle 5, provided with three drawofi' cocks, (designated 5, 5 and 5.) A still 6 is employed which is provided with means for heating it in the shape of a non-perforated coil 7, mounted within said still adjacent to the bottom and provided with a steam connection 8 and an annular spray 9, mounted and located within said still and provided with a steam connecton 10. Avalve 11, connected to the coil 7.serves as a means for draining it, and the valve 12. connected to the still 6, serves to drain the still.

A vertical column 13 about twenty feet high is connected to the top of the still 6 at 5 its lower end and to a horizontal. pipe 14 at its upper end, which pipe extends across and is connected to a vertical pipe 15, which extends downward and connects with a worm 16, mounted in a tub 17. A cross-pipe 18 7 is joined to the column 13 at a point just above the still 6 and to the pipe 15 at a point just above the worm 16. A valve 19, mounted in the column 13, controls the flow of the products of the still thcrethrough, and a valve 20, mounted in the pipe 18, serves a like purpose for it.

To enable the column 13 to be kept cool, an annular spray 21 is mounted near the top of the column and surrounds the same. A coldwater connection 22 is provided for the spray 21, and a pan 23 is located above the lower end of said column 13 and above the point at which the cross-pipe 18 is connected with the said column to catch the water dripping from 5 the spray. A pipe 21, connected to the pan 23, conducts the water caught thereby to the tub 17.

The steps of my improved process can now be set forth. The retort 1 is first filled with 9 wood, fire is then started in the furnace 2, and steam or water-vapor turned into the pipe 3. The introduction of moist steam greatly accelerates the reduction of the wood and the evaporation of the oils and is a very important step in my improved process. The disv down into the condenser 5, andthen, flows retort.

into the receptacle 5, where its specific gravity is tested. The cock 5 is opened, and the distillate permitted to flow out therethrough and into a catch-pipe 5 and is carried thereby into a suitable receptacle or directly into the still 6 as long as the specific gravity of the distillate lies between the limits 0.855 and 0.92. This comprises what I term the first fraction and is a light-yellow oil which usually passes off during the first period of from v twelve to twenty-two hours, depending upon the quality of the Wood and the size of the This fraction contains more turpentine-spirits than any of the two remaining fractions. After the first fraction has passed off the cock 5 is closed and the cock 5 opened and left open as long as the specific gravity of the outflowing oil into the catch-pipe 5 lies between 0.92 and 0.96. This comprises the second fraction and contains some woodturpentine, considerable tar and tar-oil, and some paraffin-oils, and creosote. Its average specific gravity is about 0.94. As soon as the gravity of the outflowing oil exceeds 0.96 the cock 5 is closed and the cock 5 opened and,

left open until the flow of oil into the catchpipe 5 stops. The oil last obtained comprises the third fraction and has an average gravity of about 1.015. It contains some light oils of a disagreeable odor and a large amount ofheavy paraflin-oil, suitable for lubricating purposes; but the bulk of this fraction is tar. It is owing to the elimination and separation of this third fraction from the other two that the success of my process is principally due. To separate the first fraction into its commercial products, the still 6 is filled with a charge of this first-fraction oil, steam is turned into the coil 7, the valve 20 closed, the valve 19 opened, and the water for the spray 21 turned on. The naphtha-like oils will first pass off and ascend through the column 13 and pass down into the worm 16, where they will be condensed; but the turpentine, some of which will be carried up with the water-vapor, will on encountering the cool section of the column 13 be recondensed and drop back into the still 6. The flow of naphtha-like oils will discon- .tinue after a short time, and the resulting product will have a gravity between 0. 853 and 0.858, with a pale-amber color and a strong disagreeable odor. As soon as the flow of naphtha-like oils ceases the still is shut down and permitted to cool sufficiently to be safely hanolled, after which an aqueous solution of caustic soda will be added in the proportion of from five to ten per cent. of the quantity contained in the still, which should have a gravity of about 1.20. This soda has to be added cautiously and slowly on account of the ebullition which usually takes place. As soon as the soda is added steam is again turned into the closed coil 7, and the valve 20 is opened,

after which the passing ofi? of the naphthalike oil through the column 18 will continue; but the product obtained will be mixed with turpentine, and the flow will continue but a short time. As soon as this flow ceases steam is turned into the perforated spray 9, and distillation proceeds more rapidly as the steam in combination with the turpentine from globules which ascend carry the turpentine over. The wood-spirits at this stage has a strong disagreeable odor, partaking somewhat of that of caustic soda; but the color is greatly improved and is a cloudy White. This part of the process is continued until the distillate changes color and turns to a pale amber. The oil next obtained is altogether different from the first yellow oil obtained and also from the bulk of the run, which may be considered crude turpentine, which is of a pale-amber color in the case of the first-fraction oil. To treat the second-fraction oil, identically the same process and apparatus is employed as described above in the treatment in the firstfraction oil. The products obtained differ only in the relative amounts of the heavier and lighter oils. To treat the third-fraction oil, the same apparatus is employed as above described; but certain slight changes in the manner of manipulation are made. The still 6 is first charged with third-fraction oil, after which steam is turned into the coil 7, the valve 19 opened, the valve 20 closed, and water is supplied to the spray 21. The distillation will then proceed, and a light-amber-colored oil will pass off through the column 13, which oil is practically identical with the oil obtained through the column in distilling first-fraction oil. The cooling of the column 13 causes certain greasy oils to fall back into the still. After the still ceases to run the valve 19 is closed, the valve 20 is opened, and then the distillation will continue by way of the pipe 18, but will eventually stop. At this stage of the process it has been usual in the old method of procedure to appy heatthat is, fireto the still with a consequent carbonizing and blackening of the tarry residue therein; but in my process the distillation is continued from this point by turning steam into the perforated pipe 9, thereby bringing the steam directly into the mass of tar-oil contained therein, with the result that the remaining light oil is carried over mechanically by the steam and this portion of the distillation effected rapidly. The oil brought over by the steam is very different from the first portion of the distillate obtained from the third-fraction oil and is slightly greasy to the touch and contains some trace of paraffin. The change to this fraction is made at about gravityO. 88 and the change concluded when the gravity test reaches about 0.95. The residue now remaining in the still is of a dark-brown color, perfectly adapted for all commercial purposes, and the tar is free from all dirt,

Ioo

water, or other impurities, the washing of the contents of the still by the live-steam jets having completely removed and distilled off the acid in the oils, leaving a neutral body.

I do not wish to be limited as to details of construction, as these may be modified in many particulars without departing from the spirit of my invention.

I claim 1. The art of reducing pine-wood and dividing its distillates into three fractions of graduated specific gravities which consists in filling the retort with wood and applying steam or water-vapor to the same at the same time applying heat; conducting the distillate into a receptacle where its specific gravity can be tested and continuing the process of distillation as long as the specific gravity of the distillate lies between the limits of 0.855 and 0.92; changing the discharge and catching means of the distillate and continuing the distillation until the outflowing oil or distillate lies between 0.92 and 0.96, the average being about 0. 9- then again charging the means for catching and discharging the distillate and distilling the wood completely with an outflow or distillate of an average gravity of about 1.015, substantially as hereinbefore set forth.

2. The art of reducing pine-Wood and dividing its distillates into three fractions of grad uated specific gravities which consists in filling the retort with wood and applying steam or water-vapor to the same at the same time applying heat; conducting the distillate into a receptacle where its specific gravity can be tested and continuing the process of distilla tion as long as the specific gravity of the distillate lies between the limit of 0.855 and 0.92; changing the discharge and catching means of the distillate, and continuing the distillation until the outflowing oil or distillate lies between 0.92 and 0.96, the average being 0.94:;

then again changing the means for catching and discharging the distillate and distilling the wood completely with an outflow or distillate of an average gravity of about 1.015; and subsequently distilling each of the said separate fractions substantially as hereinbefore set forth for their reduction to their final commercial products.

3. The art of distilling oils from pine-wood, which consists in first distilling crude oils directly from the wood by the application of heat in the presence of aqueous vapor, condensing the distillate during the reduction of the wood and during this act dividing it into three fractions, a first fraction with a gravity between 0.855 and 0.92; a second fraction with a gravity between 0.92 and 0.96; and a third fraction with a gravity between 0.96 and 1.00, and separating each of the said fractions of crude oils into its commercial products, by distillation through the application of heat and aqueous vapor applied within the still only at the bottom portion thereof.

In testimony whereof I have hereunto set my hand in presence of two subscribing witnesses.

JOHN CAPLES MALLONEE. WVitnesses:

J. A. AMMoNs, B. F. JORDAN. 

